JMEPEG (2021) 30:8057–8064 ÓASM International

https://doi.org/10.1007/s11665-021-05994-9 1059-9495/$19.00

Effect of Chromium Content in the Steel Substrate

on the Coating Formation and Tribological Properties
of Manganese Phosphate Coatings
Andreas Nevosad , Wolfgang Molnar, and Sabine Schwarz

Submitted: 3 December 2020 / Revised: 16 May 2021 / Accepted: 16 June 2021 / Published online: 6 July 2021

In the literature and industrial experience, the effect of insufficient and poor manganese phosphate coating
formation on steel with higher chromium content (> 1 wt%) is well known, but the reason for this
limitation or the appearance and tribological performance of such coatings is not described sufficiently.
This work describes the differences in structure and tribological properties of manganese phosphate
coatings on different steels with up to 3 wt% of chromium and reveals the formation of amorphous and
crystalline phosphate phases by transmission electron microscopy (TEM). The tribological experiments
were performed on a high load test setup with API modified as lubricant. Besides TEM also scanning
electron microscopy, and focused ion beam cross sections were employed to investigate the microstructure
and appearance of the coatings. Furthermore, this work describes the formation of tribologically superior
coatings on martensitic steel with up to 3 wt% chromium.

of metal to be coated represent the key factors affecting the

Keywords chromium phosphate, conversion coating, manganese
phosphate coating, transmission electron microscopy
1. Introduction
Phosphate conversion coatings are applied on iron and steel
surfaces for more than a century (Ref 1-3). Nowadays,
chemical and electrochemical phosphating represents a com-
monly used surface pretreatment and finishing process of
ferrous and non-ferrous metals (Ref 4-6). Due to their
combination of economical, manufacturing (e.g., speed of
operation) and physicochemical characteristics (e.g., friction
reduction, increase in wear and corrosion resistance in combi-
nation with lubrication or organic coatings), phosphate coatings
have found their application in a variety of industries, e.g.,
automotive, petroleum production and home appliances (Ref 7-
10). Most common are zinc-, iron- and manganese-phosphates,
of which manganese ones feature the most advantageous
tribological properties. In detail: hardness, excellent wear and
corrosion resistance in combination with oil, grease or lacquer
(Ref 11-15).
Phosphate coatings are usually applied by immersion, using
a series of baths, applying degreasing, rinsing and phosphating
stages, respectively. In particular, the bath composition,
together with the processing temperature (typically of 30-
99 °C), time (varying with the selected material and thickness
of the layer from seconds up to several tens of minutes) and sort
Andreas Nevosad and Wolfgang Molnar, AC2T research GmbH,
Viktor-Kaplan-Straße 2C, A-2700 Wiener Neustadt, Austria; and
Sabine Schwarz, University Service Centre for Transmission Electron
Microscopy (USTEM), Vienna University of Technology, Wiedner
Hauptstraße 8-10/057-02, A-1040 Vienna, Austria. Contact e-mail:
andreas.nevosad@ac2t.at.
phosphating process and also the composition of the phosphate
coating itself (Ref 1, 7, 16-19).
In this work, only chemically deposited manganese phos-
phate conversion coatings are considered. The deposition
process and coating growth can be described concisely as:
When steel is immersed into a the phosphatizing bath, metal
dissolution on the microanodes and generation of H2 at the
microcathodes by reaction of H3PO4 with the substrate occurs.
This causes a local depletion of free acid in the diffusion layer
at the surface of the substrate (increase in pH), which alters the
solubility of primary manganese phosphates in the bath and
leads to precipitation until a continuous coating, preferably of
hureaulite crystals ((Mn2+,Fe2+)5[PO3(OH)|PO4]2Æ4H2O), is
formed. When the coating prevents all direct contact of the
bath to the metal substrate, the reaction seizes up. Technical
phosphatizing baths typically contain, besides phosphoric acid
and primary manganese phosphate, also nitrates for accelera-
tion of the coating growth as well as catalysts and numerous
organic components to modify the growth kinetics, the grain
size, and to increase the process stability. The entire process is
explained in more detail in various works which focus on
process parameters and bath composition (Ref 1, 4, 5, 16).
Typically, these coatings are a dense and strongly adhering
layer of hureaulite crystals with a size of several lm which
form a jagged surface topology. These grains are softer than the
steel substrate and break into smaller particles and form a
smooth layer under mechanical load (Ref 12, 14) thus
providing wear resistance and reduction in coefficient of
friction. The application of manganese phosphate coating on
steel with up to 1 % of chromium is established in industrial
applications and well described in literature (Ref 1, 5, 8, 15, 20,
21). It is kind of common knowledge and stated in bath
suppliers datasheets, but not well described in scientific
literature, that a higher chromium content causes the formation
of inferior phosphate coatings or totally inhibits the formation
of a coating (Ref 1).

Journal of Materials Engineering and Performance Volume 30(11) November 2021—8057

 Aim of this work is to get a deeper insight in the formation
and tribological properties of phosphate coatings on steels with
up to 3 wt% chromium. Based on this knowledge, the
phosphatizing process was modified, which allowed to produce
a favorable Mn-phosphate coating on a steel with a chromium
content of 3 wt%.
2. Experimental
2.1 Materials and Coating Parameters
For the main coating and tribological investigations, two
heat-treatable steels in quenched and annealed condition with
similar microstructure and mechanical properties, but a differ-
ent content in chromium, were chosen as substrates for the
phosphatizing process. The two heat-treatable steels are (in
wt%): with approximately 1% Cr HT1 (0.3 C, 0.5 Mn, 0.9 Cr,
0.5 Mo, balance Fe) and with 3% Cr HT3 (0.2 C, 0.9 Mn, 3 Cr,
0.2 Mo, balance Fe).
To ensure a clean surface after cutting and grinding, the
samples were rinsed with petroleum ether, followed by another
rinse with deionized water and pickled in 0.1 M NaOH for one
minute prior to phosphatizing. The commercially available
phosphatizing solution Bonderite MN 4902 from Henkel
served as basis for the phosphatizing agent. No activation step
was performed. The concentrated Bonderite was diluted
according to specifications by 18:82 (18%) with deionized
water and possible additives were supplemented to the solution.
The bath was heated up to the desired temperature of 90 °C.
The samples were subsequently immersed in the phosphat-
ing bath for 14 minutes. By optical appearance, all samples
changed to gray color. Depending on the phosphating param-
eters, the color varied from light to dark gray with some
samples turning almost black. Afterward, the samples were
again rinsed with deionized water and dried in air.
The phosphatizing of the main samples was done on HT1 in
18% Bonderite bath (Sample ID: HT1A), HT3 in 18%
Bonderite bath (Sample ID: HT3A), and HT3 in a modified
bath (Sample ID: HT3B). To investigate the influence of
dissolved chromium, a mild steel type 1.0038 (denoted as MS;
in wt%: <0.2 C, <1.4 Mn) was phosphatized in standard
Bonderite process and an especially modified bath with added
chromium ions as 0.1 mol/l Cr(NO3)3Æ9 H2O.
Due to size and number, the specimen for the tribological
experiments was coated in an industrial phosphatizing line
including an activation step, based on the specifications of
Henkel and with the same parameters and modifications as
described above.
2.2 Tribological Experiments
The tribological experiments were performed on a machine
which incorporates a compression-tension testing machine with
a maximum axial force of 200 kN and a rotary unit driven by an
electric motor with a maximum torque of 1000 Nm. The device
is explained in detail by Cihak-Bayr et al. (Ref 22). The
experiments are similar to the ring on ring experiments
described by Ernens in (Ref 8). In contrast to these experi-
ments, we used a conical contact geometry with coated outer
and uncoated inner sample. For our experiments, a combination
of rotational movement with linearly increasing load was used.
Rotational speed was one full rotation in one minute which was
8058—Volume 30(11) November 2021
also the time until the maximum of force was reached. The
maximum contact pressure was calculated to be 2000 MPa
which is above the elastic limit of the steels and the specimen
were plastically deformed during the experiments. To determine
the durability of the coatings, cyclic experiments were per-
formed where every cycle consisted of two steps. In the first
step, after lubrication and bringing the specimen into contact, a
constantly increasing load was applied until the maximum set
force was reached, while one of the specimens made one full
rotation. In the second step, the rotation direction was reversed
and force was reduced until the specimen was again separated.
These cycles were repeated until galling was observed or the
abortion criteria of ten cycles were reached. Galling was clearly
visible as severe surface damage by optical inspection as well
as in the measured torque signal. Otherwise, the torque signal
showed no significant difference between the individual
samples and only the reached number of cycles was considered.
For each combination of steel and coating 10 sets of samples
were tested.
Only specimen made from the two heat treatable steels HT1
and HT3 with the original bath composition (A) and the altered
bath (B) were used for the tribological experiments. The
experimental setup was made up of two parts of the same
material with one part uncoated and the other coated. As
lubricant served the thread compound Bestolife Ò API
Modified which contains, according to application sheet, 18
± 1.0 wt% powdered graphite, 30.5 ± 0.6 wt% lead powder,
12.2 ± 0.6 wt% zinc dust and 3.3 ± 0.3 wt% copper flakes.
The interaction of this lubricant with manganese phosphate
coatings is well described in literature (Ref 8, 23).
2.3 Scanning Electron Microscopy
Scanning electron microscopy (SEM) images and focused
ion beam (FIB) cross sections were obtained from the
phosphated samples employing a Zeiss SUPRATM 40VP field
emission scanning electron microscope with GEMINI column.
2.4 Transmission Electron Microscopy
Thin cross sections for transmission electron microscopy
(TEM) were prepared via focused ion beam cutting on a FEI
Quanta 200 3D DBFIB.
Transmission electron microscope (TEM) investigations
were performed on a FEI Tecnai F20, equipped with an EDAX
Apollo EDX detector and a GATAN Orius 600 bottom mount
CCD for image acquisition.
3. Results and Discussion
In this section, first the results of the tribological experi-
ments are shown to demonstrate the differences in performance
of the coatings. Then, the results of the detailed investigations
of the coatings are presented.
3.1 Tribological Experiments
The tribological experiments were performed until galling
was detected after a performed cycle or 10 cycles without
galling were reached. Galling was clearly observable as severe
plastic deformation of the surface in the wear track as seen in
Fig. 1(a) as well as a sudden deviation in the torque over force
Journal of Materials Engineering and Performance
plots as seen in Fig. 1(b). These plots show first an increase in
torque signal with increasing force. At the maximum force, the
direction of the rotation is reversed and a negative torque signal
is measured which decreases with decreasing force until the
specimen are again separated. All these curves show verry little
deviation until galling occurs which was observed at different
stages of the cycle for the individual tests. More information
can not be obtained from the torque signal or the development
of the curves since no significant difference for the coatings and
individual samples was found. A calculation of the coefficient
of friction from these curves is misleading due to plastic
deformation of the samples. This is in agreement with the ring-
on-ring experiments by Ernens (Ref 8), but in contrast to these
we also saw the onset of galling in our curves. Also the
observed wear pattern is in good accordance to these exper-
iments, where also glaze layers and severe galling events with
plastic deformation of the surface were found.
A very clear statement about the tribological performance of
the coatings can be made from the number of cycles till galling,
which is depicted in Fig. 2 for each set of specimens. For the
samples with 1% Cr steel from the standard bath (HT1A) a
minimum resistance to galling with failure in the 4th cycle was
Fig. 1 Exemplary wear track with galling (a); Exemplary force-torque curve with galling event (b)
Fig. 2 Number of cycles till galling for samples and coatings HT1A, HT3A and HT3B
Journal of Materials Engineering and Performance
found (HT1A 8) and one set reached the abortion criteria of 10
cycles without galling. Set 3 for HT1A showed galling in the
10th cycle. In average, the samples from HT1A reached
approximately 6 cycles. The results for the 3% Cr steel from the
standard bath (HT3A) showed significantly less duration as
most samples failed by galling already in the second or third
cycle and only one set reached 5 cycles. Best results were found
for the 3% Cr steel samples coated in the modified bath (HT3B)
where 8 out of 10 showed no galling until the 10th cycle and
the other sets reached 8, respectively, 9 cycles. Number 1 in
HT3B was tested in an 11th cycle where galling was observed.
These results clearly demonstrate the inferior tribological
performance of phosphate coatings from a standard bath on a
steel with increased chromium content. Also the significant
improve of tribological performance due to the bath modifica-
tion is shown. The differences within the series can be
explained by inevitable deviations in the manufacturing process
and random events like contacts of asperities which start
galling. But the general performance of the series is undoubt-
edly caused by the differences in the coating.
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3.2 Detailed Investigations of the Coatings indicates very poor adhesion between phosphate layer and
substrate. The diffraction pattern in Fig. 6b, taken from the
In order to explain the differences in the tribological
region marked by a circle, indicates an amorphous nature of the
performance of the coatings detailed investigations of the
layer. The randomly oriented dots originate from small particles
coatings were performed.
which can also be observed in the TEM image itself.
3.2.1 Sample HT1A—Steel with 1% Cr, Unmodified
3.2.3 Sample MS—Mild Steel wit Chromium Added
Bath. The SEM image of the phosphated HT1A sample
in the Bath. In order to see the effect of chromium in the steel
(Fig. 3a) shows a continuous and dense phosphate layer with
and as dissolved ion in the bath, samples of an unalloyed mild
many facets and crystalline appearance as expected for such a
steel were coated in a standard bath, like HT1A and HT3A, and
manganese phosphate coating. The elemental analysis, via
a modified bath with addition of 0.1 mol/l Cr(NO3)3Æ9 H2O (see
EDX area scan, reveals phosphates, which match closely with
Fig. 7). The coating on mild steel with the original bonderite
the hureaulite formula of (Mn2+, Fe2+)5[PO3(OH)|PO4]2Æ4H2O.
composition as displayed in Fig. 7(a) resembles the coating on
The phosphates measured contain 88% manganese and
sample HT1A, which proves that a low chromium content in
12% iron as cations. The FIB cross section in (Fig. 3b)
the steel has no major influence on coating growth. The coating
shows the dense coating also in the recess between the grains.
shown in Fig. 7(b) was prepared on mild steel with addition of
Figure 4(a) shows a TEM cross section of the hureaulite
chromium nitride. This coating shows the same flat and cracked
coating and the interface between substrate and the coating on
structure as the coating on HT3B. Therefore, we can state that
sample HT1A. The coating is about 7 lm thick and two layers
dissolved chromium is responsible for the formation of this
with different microstructures can be distinguished. The upper
kind of amorphous layer and not the formation of a chromium
layer 2 is a homogenous material without pronounced defects.
oxide on the surface or other effects in the steel.
The lower area of the coating, in layer 1, exhibits a more
3.2.4 Sample HT3B—Steel with 3% Chromium, Mod-
inhomogeneous microstructure with pores (bright areas) and
ified Bath. Experiments with bath composition and various
inclusions which appear darker and consist of Fe, as proven by
additives led to the modified bath which allowed to produce
EDX analysis. These inclusions must originate from the
tribologically functional coatings also on steel with up to 3 wt%
dissolving of the substrate during the phosphatizing process
Cr (samples HT3B). This modified bath showed no change in
and therefore we conclude that the border in the coating
coating formation on samples from HT1 steel. SEM investiga-
corresponds to the former surface of the substrate.
tions of sample HT3B (Fig. 8) revealed a completely different
The diffraction pattern in Fig. 4(b) was taken from layer 2
surface compared to HT3A due to the modified bath. Here,
(indicated by the red circle in Fig. 4a) and confirmed that it
none of the amorphous, cracked, flat phase is found and instead
consists of hureaulite in good concordance with the expected
fine grained, elongated hureaulite crystals form. The larger
diffraction dots indicated in red (Fig. 4b).
hexagonal prismatic crystals in Fig. 8(a) with a length up to
3.2.2 Sample HT3A—Steel with 3% Chromium,
30 lm are precipitates from the phosphatizing bath and are
Unmodified Bath. The SEM image of the sample HT3A,
only weakly adhered to the surface. Figure 8(b) shows the
with 3% of chromium, (Fig. 5a) shows a tremendously different
finely grained structures in more detail. These crystals are also
appearance compared to the crystalline surface exhibited on
needle like prismatic with hexagonal cross section. In EDX
sample HT1A. In this case the surface consists of many flat,
measurements, no chromium was found on the surface. The
scale-like plates (5-15 lm) with gaps in between them,
FIB cross section in Fig. 8(c) shows an adhering and dense
reminding on the appearance of dry soil. The FIB cross section
coating, consisting of two layers which are further described in
in (Fig. 5b) shows that these plates are only loosely adhered to
the TEM cross sections.
the substrate and the layer is not closed. The large, crystalline
The TEM cross section in Fig. 9(a) shows a strongly
particles of hureaulite on the surface are precipitates from the
adhering coating with thickness of 6-7 lm. The holes in the
phosphatizing bath and only weakly adhered to the surface. The
specimen are caused by the thinning during preparation for
EDX measurements of the scale-like plates in Fig. 5(a) revealed
TEM. Like in sample HT1A two layers in the phosphate
a high chromium and iron content compared to the scan
coating are distinguishable by inclusions in layer 1 and a
conducted on HT1A. This means the plates consist of an iron,
homogenous structure in layer 2. The red arrow indicates the
chromium manganese phosphate.
EDX linescan which is plotted in Fig. 9(b). In the substrate
TEM investigations on sample HT3A (Fig. 6a) show a layer
mainly iron with some chromium is found. At the interface of
of 2.5-3.5 lm thickness. Also, a clear gap in the jagged
substrate and phosphate coating the concentration of Fe sharply
interface between coating and substrate can be seen. This

Fig. 3 SEM image of the sample HT1A; composition from EDX in wt%:48 O, 16 P, 32 Mn, 4 Fe (a); FIB cross section of sample HT1A (b)

8060—Volume 30(11) November 2021 Journal of Materials Engineering and Performance

Fig. 4 Cross-section TEM image of the phosphate layer on sample HT1A (a); indicated diffraction pattern of hureaulite (b)

Fig. 5 SEM image of sample HT3A; composition of flat area from EDX in wt%: 42 O, 14 P, 9 Mn,24 Fe, 10 C (a); FIB cross section of
sample HT3A (b)

Fig. 6 Cross-section TEM image of the phosphate layer on the HT3A sample (a); Diffraction pattern (b)

declines, but a slight increase in Cr concentration can be seen.
In the first two lm of the coating, a significant content of
chromium content and iron are measured. This corresponds
well with the observed layer 1. In layer 2, no chromium is
found and the content of iron and phosphorus stay at a constant
level. A steady increase in manganese and decrease in oxygen
toward the surface of the measured crystal are observed.
For a detailed analysis of the crystallographic structure of
sample HT3B, a diffraction pattern analysis was performed at
five different measurement spots which are indicated by red
circles and Greek letters in Fig. 10(a). Spot a (Fig. 10b) shows
the diffraction pattern from the substrate. It reveals a polycrys-
talline material, as expected from the employed martensitic
steel. Spot b in Fig. 10(c) features a diffraction pattern with
very few and irregular reflexes and diffuse concentric rings,
which indicates amorphous material. A similar appearance is
found at spot c (Fig. 10d), where diffuse rings appear, but also
diffraction peaks are present which originate from steel

Journal of Materials Engineering and Performance Volume 30(11) November 2021—8061

Fig. 7 Mild steel with standard coating (a); mild steel with chromium nitride added to the bath (b)

Fig. 8 SEM image of the HT3B sample; composition from EDX in wt%:30 O, 16 P, 42 Mn, 6 Fe (a); Detail of the fine-grained structure (b);
FIB cross section (c)

Fig. 9 EDX line scan over the phosphate (a); relative elemental composition of the layer depending on the position (b). The red arrow marks
the scan direction.

particles in the coating. Spots d and e in Fig. 10(e) and (f) show
no diffuse ring, but only crystalline material. Diffraction
patterns taken from point e, which represents the highest
measured point in the phosphate layer, show crystallinity und
also a good coincidence with the expected hureaulite lattice
(indicated by red dots). This proves that despite the altered
appearance of the crystals hureaulite forms in the modified
bath.
4. Summary and Conclusions
Tribological experiments demonstrated an inferior perfor-
mance of standard manganese phosphate coatings on steels
with 3 wt% Cr. Therefore, the coatings were investigated in
detail. On steel substrates up to 1 wt% of chromium (sample
HT1A and mild steel), the standard phosphatizing process
forms a dense coating of hureaulite crystals. The low Cr content
seems to have no detrimental effect on layer growth. At a
chromium content of 3 wt% in the steel substrate with a
standard phosphatizing bath (sample HT3A) no hureaulite
forms and a highly amorphous, chromium-rich phosphate is
deposited onto the surface. This layer shows cracks and poor
adhesion with a visible gap at the interface between phosphate
layer and substrate. The same coating formation resulted also
on unalloyed steel by the addition of chromium ions to the bath.
This effect of chromium and the formation of such coatings is,
to the authors actual knowledge, not described in literature. By
modifying the phosphating bath, it was possible to produce a
dense and strongly adhering, partly crystalline coating on 3
wt% Cr steel (sample HT3B). Crystalline hureaulite and
amorphous phases in this coating were proven by TEM
diffraction pattern.

8062—Volume 30(11) November 2021 Journal of Materials Engineering and Performance

Fig. 10 Cross-section TEM-image with measurement points (a); Diffraction pattern of the substrate (b); of the lower layer 1 (c-e); of the more
crystalline upper layer 2 (f)
The authors developed the following explanation for the
observed coating formation:
During the phosphatizing process, chromium gets dissolved
from the steel and is enriched in the diffusion layer where the
substrate dissolution and the coating growth occurs. A critical
amount of Cr-ions in the solution interferes with the various
simultaneous processes and instead of crystalline hureaulite an
amorphous phase forms and no passivation of the surface
happens. The bath modification on sample HT3B altered the
processes ongoing during deposition in a way that hureaulite
crystals can grow and the surface reaches the state of
passivation. In this way a strongly adhering and crystalline
hureaulite coating is formed. Nevertheless, still some amor-
phous phase is formed especially close to the substrate.
Additional effect is the formation of elongated hureaulite
crystals which was observed only on 3% Cr substrate.
These differences in coating formation explain also the
inferior tribological performance of HT3A compared to HT1A
and HT3B. The wear mechanism of crystalline manganese
phosphate coating in combination with API modified grease is
well described in the literature (Ref 8, 23). Under tribological
stress, the hureaulite crystals start to crumble and form with
incorporation of the solid lubricant particles a smooth glace
layer which prevents the surfaces from galling. On the contrary,
the coating on HT3A samples is not as strongly adhering and
also the surface structure does not promote the incorporation of
solid lubricant particles.
Journal of Materials Engineering and Performance
Acknowledgements
The authors want to thank voestalpine Tubulars Kindberg for
the support and provision of knowledge in the field of industrial
application of the manganese phosphating.
Funding
Presented results were realized in research projects with
financial support from the participating project partners and the
Austrian COMET program (Project InTribology, No. 872176). The
COMET program is funded by the Austrian Federal Government
and concerning InTribology by the provinces of Lower Austria and
Vorarlberg.
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